CN110229984B - High-strength Mg-Gd-Er-Y magnesium alloy and preparation method thereof - Google Patents

High-strength Mg-Gd-Er-Y magnesium alloy and preparation method thereof Download PDF

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CN110229984B
CN110229984B CN201910538114.4A CN201910538114A CN110229984B CN 110229984 B CN110229984 B CN 110229984B CN 201910538114 A CN201910538114 A CN 201910538114A CN 110229984 B CN110229984 B CN 110229984B
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magnesium
alloy
temperature
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melt
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CN110229984A (en
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张秋
刘文才
吴国华
张亮
周北平
肖然
丁文江
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Shanghai Jiaotong University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making alloys
    • C22C1/02Making alloys by melting
    • C22C1/03Making alloys by melting using master alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C23/00Alloys based on magnesium
    • C22C23/06Alloys based on magnesium with a rare earth metal as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/002Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/06Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon

Abstract

The invention provides a high-strength Mg-Gd-Er-Y magnesium alloy and a preparation method thereof, wherein the alloy comprises the following components in percentage by mass: 4-15 wt.% Gd, 0.2-6 wt.% Er, 0.2-6 wt.% Y, 0-4 wt.% Ho, 0-1 wt.% Zr, and Gd + Er + Y + Ho: 6.2-20 wt.%, the balance being Mg and unavoidable impurities. The preparation method of the magnesium alloy comprises three stages of smelting, thermal deformation and aging treatment. According to the invention, through thermal deformation treatment and subsequent aging treatment, partial recrystallization is carried out under the condition of keeping the texture to realize grain refinement, a recrystallization texture and a texture dual-phase structure are formed, and simultaneously, a dispersed strengthening phase is precipitated in the aging process, so that the wrought magnesium alloy has excellent room-temperature and high-temperature mechanical properties through the comprehensive effects of texture strengthening, fine grain strengthening and precipitation strengthening.

Description

High-strength Mg-Gd-Er-Y magnesium alloy and preparation method thereof
Technical Field
The invention belongs to the technical field of metal materials, relates to a high-strength magnesium alloy and a preparation method thereof, and particularly relates to a high-strength Mg-Gd-Er-Y magnesium alloy and a preparation method thereof.
Background
The magnesium alloy is used as the lightest metal structure material at present, has a series of unique advantages of high specific strength and specific rigidity, good damping vibration attenuation, strong electromagnetic shielding and heat conducting performance, easy cutting and processing, easy recovery and the like, and has great application potential in structural part industries such as aerospace, automobiles, computers, communication, consumer electronics and the like. However, the magnesium alloy has low absolute strength, poor plasticity, poor heat resistance and other defects, which severely limit the application of the magnesium alloy in the field of practical engineering.
The Mg-Al series wrought magnesium alloy is the most widely used magnesium alloy system at present, has good casting performance and can be strengthened by heat treatment, but has poor mechanical performance at room temperature, and simultaneously, the main strengthening phase Mg at high temperature17Al12Is easily coarsened, resulting in poor mechanical properties at high temperatures.
Therefore, improvement of strength and heat resistance of magnesium alloys is an important issue in the development of magnesium alloy materials. The technical personnel for optimizing the components and the heat treatment process of the magnesium alloy and developing a high-strength heat-resistant magnesium alloy become the magnesium alloy urgently to solve the problems.
The invention patent application with publication number 107245619A discloses an ultrahigh-strength high-temperature-resistant magnesium alloy, which comprises the following components in percentage by mass: gd: 8.0-9.6%, Y: 1.8-3.2%, and the ratio of Gd content to Y content is: Gd/Y is more than or equal to 3 and less than or equal to 5, and Zr: 0.3-0.7%, Ag: 0.02-0.5%, Er: 0.02-0.3%, the ratio of Ag content to Er content is: Ag/Er is more than or equal to 1 and less than or equal to 3, wherein Fe is less than or equal to 0.02 percent, Si is less than or equal to 0.02 percent, Cu is less than or equal to 0.005 percent, Ni is less than or equal to 0.003 percent, the total content of impurities is less than or equal to 0.1 percent, and the balance is Mg. In the patent, a large-size ingot with the diameter of 300-630mm can be prepared by adding Ag and Er, and a component with the outer diameter of 1700mm is prepared; the tensile strength of the alloy in a T6 state is more than or equal to 470MPa, and the yield strength is more than or equal to 400 MPa; the tensile strength at 200 ℃ is more than or equal to 350MPa, and the yield strength is more than or equal to 260 MPa. However, in this magnesium alloy, the addition of Ag causes a decrease in the solubility of rare earth elements such as Gd and Y in the magnesium alloy, a large amount of eutectic structures remain after homogenization treatment of the alloy, and the thermoplastic workability deteriorates.
Disclosure of Invention
Aiming at the problems of low strength and poor heat resistance of the existing magnesium alloy, the invention aims to provide a high-strength Mg-Gd-Er-Y magnesium alloy and a preparation method thereof. The prepared magnesium alloy is partially recrystallized by controlling the content and proportion of rare earth elements of the magnesium alloy, thermal deformation process parameters and aging treatment parameters, crystal grains are refined while a part of texture is kept, and the mechanical property of the alloy is further improved by the corresponding aging treatment process.
The purpose of the invention is realized by the following technical scheme:
the invention provides a high-strength Mg-Gd-Er-Y magnesium alloy which comprises the following elements in percentage by weight: gd is 4-15 wt.%, Er is 2-6 wt.%, Y is 0.2-6 wt.%, Ho is 0-4 wt.%, Zr is 0-1 wt.%, and the total amount of Gd, Er, Y and Ho is: 6.2-20 wt.%, the balance being Mg and unavoidable impurities.
Preferably, in the magnesium alloy, Ho is 0.5-2 wt.%. The precipitation strengthening effect of the Ho element is not as good as that of Gd, Y and Er elements, but the improvement of the plasticity of the alloy is facilitated, and the excellent comprehensive mechanical property of the alloy is ensured.
Preferably, in the magnesium alloy, Zr is 0.5-1 wt.%. The Zr element mainly plays a role in refining grains in the magnesium alloy, but when the Zr content is too high, the residual Zr core can adversely affect the mechanical properties of the alloy.
The invention also provides a preparation method of the high-strength Mg-Gd-Er-Y magnesium alloy, which comprises the three processes of smelting, thermal deformation treatment and aging treatment in sequence.
Preferably, the smelting comprises the following specific steps:
s1, baking materials: preheating pure magnesium and intermediate alloys of magnesium-gadolinium, magnesium-erbium, magnesium-yttrium, magnesium-holmium and magnesium-zirconium at the temperature of 200-240 ℃;
s2, melting magnesium, adding Gd, Er, Y and Ho: melting the dried pure magnesium in a protective atmosphere; after pure magnesium is completely melted, adding Mg-Gd intermediate alloy, Mg-Er intermediate alloy, Mg-Y intermediate alloy and Mg-Ho intermediate alloy when the temperature of the melt is raised to 730-750 ℃; wherein the addition of Gd, Er, Y and Ho is determined according to the mass percentage of Gd, Er, Y and Ho in the Mg-Gd intermediate alloy, the Mg-Er intermediate alloy, the Mg-Y intermediate alloy and the Mg-Ho intermediate alloy and the smelting yield of Gd, Er, Y and Ho elements respectively;
s3, adding Zr: under a protective atmosphere, adding an Mg-Zr intermediate alloy when the temperature of the melt obtained in the step S2 reaches 750-780 ℃, wherein the adding amount is determined according to the mass percentage of Gd in the Mg-Gd intermediate alloy and the smelting yield of Gd element;
s4, casting: and under a protective atmosphere, stirring when all alloys are completely melted and the temperature of the melt rises to 730-750 ℃, then refining without power failure for 5-10 minutes when the temperature of the melt rises to 750-760 ℃, heating to 780 ℃ after refining, standing for 25-40 minutes, skimming the surface scum after the melt is cooled to 710-740 ℃ after standing, and casting to obtain the alloy ingot.
Preferably, in step S1, the preheating time is 4 hours or more.
Preferably, in step S2, after pure magnesium is completely melted, Mg-Gd intermediate alloy, Mg-Er intermediate alloy, Mg-Y intermediate alloy and Mg-Ho intermediate alloy are added in sequence when the temperature of the melt is raised to 730-750 ℃.
Preferably, the protective atmosphere is SF6And CO2The mixed atmosphere of (3).
Preferably, in step S4, the casting steel mold is preheated to 200 to 240 ℃.
Preferably, the thermal deformation treatment comprises the following specific steps:
a1, carrying out solid solution on the alloy ingot obtained by smelting at 480-540 ℃ for 2-10 hours in advance, and quenching with warm water at 70 ℃;
a2, carrying out hot extrusion on the cast ingot subjected to the solution treatment in the step A1, wherein the extrusion temperature is 200 ℃, and the extrusion ratio is 20: 1.
Preferably, the aging treatment comprises the following specific steps: aging for 2-10 h at 170-250 ℃, and then aging for 10-60 h at 100-170 ℃. The first-stage aging temperature is higher, the time is shorter, a large amount of nucleation of a precipitated phase can be promoted, the second-stage aging temperature is lower, the time is longer, the further growth of the precipitated phase can be promoted, the precipitated phase can be uniformly dispersed in a matrix through the two-stage aging treatment, and the alloy is guaranteed to have good mechanical properties.
According to the invention, through solid solution treatment, thermal deformation treatment and subsequent aging treatment, partial recrystallization is carried out under the condition of keeping the texture to realize grain refinement, a recrystallized structure and a texture dual-phase structure are formed, meanwhile, the alloy strength is further improved through a dispersion strengthening phase precipitated in the aging process, and the magnesium alloy has excellent room-temperature and high-temperature mechanical properties through the comprehensive effects of texture strengthening, fine-grain strengthening and precipitation strengthening.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, other rare earth elements are added on the basis of the traditional Mg-Gd-Y alloy, so that the room temperature strength, plasticity and heat resistance of the alloy are improved.
2. The invention can partially recrystallize the wrought magnesium alloy by carrying out hot extrusion treatment and subsequent aging treatment on the magnesium alloy, so that the alloy has a two-phase structure of texture and recrystallized grains, and has better comprehensive mechanical properties compared with the wrought alloy which is completely recrystallized.
3. The invention also provides a heat treatment method of double-stage aging, which promotes the precipitation of dispersed phases under the condition of ensuring that recrystallized grains are not obviously grown, and further improves the mechanical property of the alloy.
4. In the application, the Ho element is added, the atomic radius of the Ho element is close to that of Gd, Er and Y elements, and the damage to the plasticity of the alloy is small in the aging precipitation process.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be obvious to those skilled in the art that various changes and modifications can be made without departing from the spirit of the invention. All falling within the scope of the present invention.
The following embodiment provides a high-strength Mg-Gd-Er-Y magnesium alloy and a preparation method thereof, wherein the high-strength Mg-Gd-Er-Y magnesium alloy comprises the following components in percentage by mass: 4-15 wt.% Gd, 0.2-6 wt.% Er, 0.2-6 wt.% Y, 0-4% Ho, Zr content of 0-1 wt.%, Gd + Er + Y + Ho: 6.2-20 wt.%, the balance being Mg and unavoidable impurities. The wt.% refers to the percentage of the component in the total mass of the alloy formulated.
Gd is adopted as a first component, because the solid solubility of the Gd in an Mg solid solution is 3.82 wt% at 200 ℃, the addition amount of the Gd is not lower than 4 wt% for ensuring that the alloy obtains good effects of aging precipitation strengthening and solid solution strength, and meanwhile, the addition amount of the Gd is not higher than 15 wt% for avoiding too much increase of the alloy cost and density and excessive embrittlement of the alloy; er, Y and Ho are used as the second, third and fourth components, so that the solid solubility of Gd in Mg can be reduced, the aging precipitation strengthening effect of Gd is improved, and the appearance of an aging hardness peak value can be advanced. Meanwhile, in order to reduce the cost, the addition amount of the rare earth elements is not excessively high, and Gd + Y + Er + Ho is in a range of 6.2 to 20 wt.%. Zr is adopted as a fourth component to improve the toughness of the alloy and improve the processing property of the alloy.
The preparation method of the high-strength wrought magnesium alloy Mg-Gd-Er-Y is divided into three stages, and comprises the steps of smelting, thermal deformation and subsequent heat treatment in sequence; wherein the content of the first and second substances,
the smelting process is carried out in SF6And CO2The method is carried out under the protection of mixed gas, and comprises the following steps:
(1) drying materials: preheating pure magnesium, magnesium-gadolinium, magnesium-erbium, magnesium-yttrium, magnesium-holmium and magnesium-zirconium intermediate alloy at 200-240 ℃ for 4 hours;
(2) melting magnesium: under the protective atmosphere, adopting a resistance furnace to melt the dried pure magnesium;
(3) adding Gd: under a protective atmosphere, after pure magnesium is completely melted, adding Mg-Gd intermediate alloy when the temperature of the melt is raised to 730-750 ℃, wherein the adding amount is determined according to the mass percentage of Gd in the Mg-Gd intermediate alloy and the smelting yield of Gd element;
(4) adding Er, Y and Ho: under a protective atmosphere, after Mg-Gd is melted, adding a Mg-Er intermediate alloy when the temperature of the melt is raised to 730-750 ℃, wherein the adding amount is determined according to the mass percentage of Er in the Mg-Er intermediate alloy and the smelting yield of Er element; in this way, Mg-Y, Mg-Ho was added;
(5) adding Zr: adding Mg-Zr intermediate alloy when the temperature of the melt reaches 750-780 ℃ under the protective atmosphere, wherein the adding amount is determined according to the mass percentage of Zr in the Mg-Zr intermediate alloy and the smelting yield of Zr element;
(6) casting: and stirring for 5 minutes when all the alloys are completely melted and the temperature of the melt rises to 730-750 ℃, then refining for 5-10 minutes without power failure when the temperature of the melt rises to 750-760 ℃, heating to 780 ℃ after refining, standing for 25-40 minutes, skimming the surface scum and casting into alloy ingots after the melt is cooled to 710-740 ℃, and preheating a steel mould for casting to 200-240 ℃.
The thermal deformation process comprises the following steps:
(1) and (3) carrying out solid solution treatment on the alloy ingot obtained by smelting at 480-540 ℃ for 2-10 hours in advance, and quenching with warm water at 70 ℃.
(2) Carrying out hot extrusion on the cast ingot subjected to the solution treatment, wherein the extrusion temperature is 200 ℃, and the extrusion ratio is 20: 1.
the aging treatment process comprises the following steps:
aging for 2-10 h at 170-250 ℃, and then aging for 10-60 h at 100-170 ℃. And carrying out water quenching treatment after aging.
Example 1
The embodiment provides a high-strength Mg-Gd-Er-Y magnesium alloy which comprises the following components in percentage by mass: 15 wt.% Gd, 3 wt.% Er, 2 wt.% Y, 1 wt.% Zr, the balance Mg and unavoidable impurities, the total amount of impurity elements Si, Fe, Cu and Ni being less than 0.02 wt.%.
The preparation method of the Mg-Gd-Er-Y magnesium alloy comprises the following steps:
1. melting
At SF6And CO2The method is carried out under the protection of mixed gas, and comprises the following steps:
(1) drying materials: preheating pure magnesium, magnesium-gadolinium, magnesium-erbium, magnesium-yttrium and magnesium-zirconium intermediate alloy for 4 hours at 200 ℃;
(2) melting magnesium: under the protective atmosphere, adopting a resistance furnace to melt the dried pure magnesium;
(3) adding Gd: under the protective atmosphere, after pure magnesium is completely melted, adding Mg-Gd intermediate alloy when the temperature of the melt is raised to 750 ℃, wherein the adding amount is determined according to the mass percentage of Gd in the Mg-Gd intermediate alloy and the smelting yield of Gd element;
(4) adding Er, Y: under the protective atmosphere, after Mg-Gd is melted, adding Mg-Er intermediate alloy when the temperature of the melt is raised to 750 ℃; adding Mg-Y according to the mode;
(5) adding Zr: adding Mg-Zr intermediate alloy when the temperature of the melt reaches 780 ℃ in protective atmosphere;
(6) casting: stirring for 5 minutes when all alloys are completely melted and the temperature of the melt rises to 750 ℃, then continuously refining for 10 minutes when the temperature of the melt rises to 760 ℃, heating to 780 ℃ after refining, standing for 30 minutes, skimming surface scum and casting into alloy ingots after the melt is cooled to 720 ℃, and preheating a steel mould for casting to 200 ℃.
2. Heat distortion treatment
(1) Pre-dissolving an alloy ingot obtained by smelting at 540 ℃ for 10 hours, and quenching with warm water at 70 ℃;
(2) carrying out hot extrusion on the cast ingot subjected to the solution treatment, wherein the extrusion temperature is 200 ℃, and the extrusion ratio is 20: 1.
3. aging treatment
Carrying out aging treatment on the alloy obtained after thermal deformation, wherein the aging process comprises the following steps: aging at 250 deg.C for 10 hr, and aging at 170 deg.C for 60 hr. And carrying out water quenching treatment after aging.
The mechanical properties of the high-strength wrought magnesium rare earth alloy prepared by the embodiment are as follows: room temperature: the yield strength is 307.4MPa, the tensile strength is 340.6MPa, and the elongation is 5.6%. High temperature 150 ℃ of: the yield strength is 252.4MPa, the tensile strength is 283.6MPa, and the elongation is 8.4%.
Example 2
The embodiment provides a high-strength Mg-Gd-Er-Y magnesium alloy which comprises the following components in percentage by mass: 10 wt.% Gd, 5 wt.% Er, 3 wt.% Y, 2 wt.% Ho, 0.5 wt.% Zr, the balance Mg and unavoidable impurities, the total amount of impurity elements Si, Fe, Cu and Ni being less than 0.02 wt.%.
1. Melting
At SF6And CO2The method is carried out under the protection of mixed gas, and comprises the following steps:
(1) drying materials: preheating pure magnesium, magnesium-gadolinium, magnesium-erbium, magnesium-yttrium, magnesium-holmium and magnesium-zirconium intermediate alloy for 4 hours at 200 ℃;
(2) melting magnesium: under the protective atmosphere, adopting a resistance furnace to melt the dried pure magnesium;
(3) adding Gd: under the protective atmosphere, after pure magnesium is completely melted, adding Mg-Gd intermediate alloy when the temperature of the melt is raised to 750 ℃, wherein the adding amount is determined according to the mass percentage of Gd in the Mg-Gd intermediate alloy and the smelting yield of Gd element;
(4) adding Er, Y and Ho: under the protective atmosphere, after Mg-Gd is melted, adding Mg-Er intermediate alloy when the temperature of the melt is raised to 750 ℃; in this way, Mg-Y, Mg-Ho was added;
(5) adding Zr: adding Mg-Zr intermediate alloy when the temperature of the melt reaches 780 ℃ in protective atmosphere;
(6) casting: and (3) stirring for 5 minutes when all the alloys are completely melted and the temperature of the melt rises to 750 ℃, then refining for 10 minutes without power off when the temperature of the melt rises to 750-760 ℃, heating to 780 ℃ after refining, standing for 30 minutes, skimming the surface scum and casting into alloy ingots after the melt is cooled to 720 ℃, and preheating to 200 ℃ by using a steel mould for casting.
2. Heat distortion treatment
(1) The alloy ingot obtained by smelting is subjected to solid solution for 8 hours at the temperature of 520 ℃ in advance, and is quenched by warm water at the temperature of 70 ℃.
(2) And carrying out hot extrusion on the cast ingot after the solution treatment, wherein the extrusion temperature is 200 ℃, and the extrusion ratio is 20: 1.
3. Aging treatment
Carrying out aging treatment on the alloy obtained after thermal deformation, wherein the aging process comprises the following steps: aging at 250 deg.C for 10 hr, and aging at 170 deg.C for 60 hr. And carrying out water quenching treatment after aging.
The mechanical properties of the high-strength wrought magnesium rare earth alloy prepared by the embodiment are as follows: room temperature: the yield strength was 480.6MPa, the tensile strength was 520.0MPa, and the elongation was 5.6%. High temperature 150 ℃ of: the yield strength is 504MPa, the tensile strength is 536.8MPa, and the elongation is 7.8%.
Example 3
The embodiment provides a high-strength Mg-Gd-Er-Y magnesium alloy which comprises the following components in percentage by mass: 4 wt.% Gd, 2 wt.% Er, 2 wt.% Y, 2 wt.% Ho, 0.5 wt.% Zr, the balance Mg and unavoidable impurities, the total amount of impurity elements Si, Fe, Cu and Ni being less than 0.02 wt.%.
1. Melting
At SF6And CO2The method is carried out under the protection of mixed gas, and comprises the following steps:
(1) drying materials: preheating pure magnesium, magnesium-gadolinium, magnesium-erbium, magnesium-yttrium, magnesium-holmium and magnesium-zirconium intermediate alloy for 4 hours at 200 ℃;
(2) melting magnesium: under the protective atmosphere, adopting a resistance furnace to melt the dried pure magnesium;
(3) adding Gd: under the protective atmosphere, after pure magnesium is completely melted, adding Mg-Gd intermediate alloy when the temperature of the melt is raised to 750 ℃, wherein the adding amount is determined according to the mass percentage of Gd in the Mg-Gd intermediate alloy and the smelting yield of Gd element;
(4) adding Er, Y and Ho: under the protective atmosphere, after Mg-Gd is melted, adding Mg-Er intermediate alloy when the temperature of the melt is raised to 750 ℃; in this manner, Mg-Y, Mg-Ho was added.
(5) Adding Zr: adding Mg-Zr intermediate alloy when the temperature of the melt reaches 780 ℃ in protective atmosphere
(6) Casting: stirring for 5 minutes when all alloys are completely melted and the temperature of the melt rises to 750 ℃, then continuously refining for 10 minutes when the temperature of the melt rises to 760 ℃, heating to 780 ℃ after refining, standing for 30 minutes, skimming surface scum and casting into alloy ingots after the melt is cooled to 720 ℃, and preheating a steel mould for casting to 200 ℃.
2. Heat distortion treatment
(1) The alloy ingot obtained by smelting is subjected to solid solution for 20 hours at 500 ℃ in advance, and is quenched by warm water at 70 ℃.
(2) Carrying out hot extrusion on the cast ingot subjected to the solution treatment, wherein the extrusion temperature is 200 ℃, and the extrusion ratio is 20: 1.
3. aging treatment
Carrying out aging treatment on the alloy obtained after thermal deformation, wherein the aging process comprises the following steps: aging at 200 deg.C for 8 hr, and aging at 150 deg.C for 20 hr. And carrying out water quenching treatment after aging.
The mechanical properties of the high-strength wrought magnesium rare earth alloy prepared by the embodiment are as follows: room temperature: the yield strength was 350.6MPa, the tensile strength was 390.6MPa, and the elongation was 12.6%. High temperature 150 ℃ of: the yield strength was 346.2MPa, the tensile strength was 356MPa, and the elongation was 15.3%.
Example 4
The embodiment provides a high-strength Mg-Gd-Er-Y magnesium alloy which comprises the following components in percentage by mass: 4 wt.% Gd, 2 wt.% Er, 0.2 wt.% Y, 4 wt.% Ho, 0.1 wt.% Zr, the balance Mg and unavoidable impurities, the total amount of impurity elements Si, Fe, Cu and Ni being less than 0.02 wt.%.
1. Melting
At SF6And CO2The method is carried out under the protection of mixed gas, and comprises the following steps:
(1) drying materials: preheating pure magnesium, magnesium-gadolinium, magnesium-erbium, magnesium-yttrium, magnesium-holmium and magnesium-zirconium intermediate alloy for 4 hours at 200 ℃;
(2) melting magnesium: under the protective atmosphere, adopting a resistance furnace to melt the dried pure magnesium;
(3) adding Gd: under the protective atmosphere, after pure magnesium is completely melted, adding Mg-Gd intermediate alloy when the temperature of the melt is raised back to 730 ℃, wherein the adding amount is determined according to the mass percentage of Gd in the Mg-Gd intermediate alloy and the smelting yield of Gd element;
(4) adding Er, Y and Ho: under the protective atmosphere, after Mg-Gd is melted, adding Mg-Er intermediate alloy when the temperature of the melt is raised back to 730 ℃; in this manner, Mg-Y, Mg-Ho was added.
(5) Adding Zr: adding Mg-Zr intermediate alloy when the temperature of the melt reaches 760 ℃ in the protective atmosphere
(6) Casting: and (3) stirring for 5 minutes when all the alloys are completely melted and the temperature of the melt rises to 750 ℃, then refining for 8 minutes without power off when the temperature of the melt rises to 750-760 ℃, heating to 780 ℃ after refining, standing for 25 minutes, skimming the surface scum and casting into alloy ingots after the melt is cooled to 710 ℃, and preheating to 240 ℃ by using a steel mould for casting.
2. Heat distortion treatment
(1) The alloy ingot obtained by smelting is subjected to solid solution for 2 hours at 500 ℃ in advance, and is quenched by warm water at 70 ℃.
(2) Carrying out hot extrusion on the cast ingot subjected to the solution treatment, wherein the extrusion temperature is 200 ℃, and the extrusion ratio is 20: 1.
3. aging treatment
Carrying out aging treatment on the alloy obtained after thermal deformation, wherein the aging process comprises the following steps: aging at 200 deg.C for 2h, and aging at 150 deg.C for 20 h. And carrying out water quenching treatment after aging.
The mechanical properties of the high-strength wrought magnesium rare earth alloy prepared by the embodiment are as follows: room temperature: the yield strength is 319.4MPa, the tensile strength is 360.9MPa, and the elongation is 8.6%. High temperature 150 ℃ of: the yield strength is 262.9MPa, the tensile strength is 293.4MPa, and the elongation is 10.4%.
Example 5
The embodiment provides a high-strength Mg-Gd-Er-Y magnesium alloy which comprises the following components in percentage by mass: 4 wt.% Gd, 6 wt.% Er, 6 wt.% Y, 0.5 wt.% Ho, 0.1 wt.% Zr, the balance Mg and unavoidable impurities, the total amount of impurity elements Si, Fe, Cu and Ni being less than 0.02 wt.%.
1. Melting
At SF6And CO2The method is carried out under the protection of mixed gas, and comprises the following steps:
(1) drying materials: preheating pure magnesium, magnesium-gadolinium, magnesium-erbium, magnesium-yttrium, magnesium-holmium and magnesium-zirconium intermediate alloy for 4 hours at 200 ℃;
(2) melting magnesium: under the protective atmosphere, adopting a resistance furnace to melt the dried pure magnesium;
(3) adding Gd: under the protective atmosphere, after pure magnesium is completely melted, adding Mg-Gd intermediate alloy when the temperature of the melt is raised to 740 ℃, wherein the adding amount is determined according to the mass percentage of Gd in the Mg-Gd intermediate alloy and the smelting yield of Gd element;
(4) adding Er, Y and Ho: under the protective atmosphere, after Mg-Gd is melted, adding Mg-Er intermediate alloy when the temperature of the melt is raised to 740 ℃; in this manner, Mg-Y, Mg-Ho was added.
(5) Adding Zr: under the protective atmosphere, adding Mg-Zr intermediate alloy when the temperature of the melt reaches 750 DEG C
(6) Casting: and (3) stirring for 5 minutes when all the alloys are completely melted and the temperature of the melt rises to 740 ℃, then continuously refining for 5 minutes when the temperature of the melt rises to 750-760 ℃, heating to 780 ℃ after refining, standing for 40 minutes, skimming the surface scum and casting into alloy ingots after the melt is cooled to 740 ℃ after standing, and preheating to 220 ℃ by using a steel mould for casting.
2. Heat distortion treatment
(1) The alloy ingot obtained by smelting is subjected to solid solution for 2 hours at 500 ℃ in advance, and is quenched by warm water at 70 ℃.
(2) Carrying out hot extrusion on the cast ingot subjected to the solution treatment, wherein the extrusion temperature is 200 ℃, and the extrusion ratio is 20: 1.
3. aging treatment
Carrying out aging treatment on the alloy obtained after thermal deformation, wherein the aging process comprises the following steps: aging at 200 deg.C for 2h, and aging at 150 deg.C for 20 h. And carrying out water quenching treatment after aging.
The mechanical properties of the high-strength wrought magnesium rare earth alloy prepared by the embodiment are as follows: room temperature: the yield strength is 320.4MPa, the tensile strength is 380.4MPa, and the elongation is 7.6%. High temperature 150 ℃ of: the yield strength is 300.5MPa, the tensile strength is 340.6MPa, and the elongation is 12.6%.
Example 6
The embodiment provides a high-strength Mg-Gd-Er-Y magnesium alloy, which is basically consistent with the embodiment 5 in percentage by mass, and is different from the embodiment only in that: in this example, Zr is 1 wt.%, that is, the mass percentages of the components are: 4 wt.% Gd, 6 wt.% Er, 6 wt.% Y, 0.5 wt.% Ho, 1 wt.% Zr, the balance Mg and unavoidable impurities, the total amount of impurity elements Si, Fe, Cu and Ni being less than 0.02 wt.%. The preparation method of the magnesium rare earth alloy in the embodiment is the same as that of the embodiment 5.
The mechanical properties of the magnesium rare earth alloy prepared by the embodiment are as follows: room temperature: the yield strength was 356.7MPa, the tensile strength was 371.2MPa, and the elongation was 10.6%. High temperature 150 ℃ of: the yield strength is 294.7MPa, the tensile strength is 330.6MPa, and the elongation is 15.4%.
Comparative example 1
The comparative example provides a magnesium rare earth alloy, which is basically consistent with example 4 in all the components in percentage by mass, and is different only in that: in the comparative example, no Er element is added, and the mass percent of each component is as follows: 4 wt.% Gd, 0.2 wt.% Y, 4 wt.% Ho, 0.1 wt.% Zr, the balance Mg and unavoidable impurities, the total amount of impurity elements Si, Fe, Cu and Ni being less than 0.02 wt.%. The preparation method of the magnesium rare earth alloy in the comparative example is consistent with that of example 4.
The mechanical properties of the magnesium rare earth alloy prepared by the comparative example are as follows: room temperature: the yield strength is 223.5MPa, the tensile strength is 260.5MPa, and the elongation is 8.6%. High temperature 150 ℃ of: the yield strength is 209.5MPa, the tensile strength is 235.9MPa, and the elongation is 10.8%.
Comparative example 2
The comparative example provides a magnesium rare earth alloy, which is basically consistent with example 4 in all the components in percentage by mass, and is different only in that: the Y element is not added in the comparative example, and the mass percentages of the components are as follows: 4 wt.% Gd, 2 wt.% Er, 4 wt.% Ho, 0.1 wt.% Zr, the balance being Mg and unavoidable impurities, the total amount of impurity elements Si, Fe, Cu and Ni being less than 0.02 wt.%. The preparation method of the magnesium rare earth alloy in the comparative example is consistent with that of example 4.
The mechanical properties of the magnesium rare earth alloy prepared by the comparative example are as follows: room temperature: the yield strength was 230.2MPa, the tensile strength was 275.4MPa, and the elongation was 8.7%. High temperature 150 ℃ of: the yield strength was 206.4MPa, the tensile strength was 259.4MPa, and the elongation was 11.8%.
Comparative example 3
The present comparative example provides a magnesium rare earth alloy having the components in the mass percentages consistent with example 4, with specific alloy compositions of 4 wt.% Gd, 2 wt.% Er, 0.2 wt.% Y, 4 wt.% Ho, 0.1 wt.% Zr, the balance Mg and unavoidable impurities, and the total amount of impurity elements Si, Fe, Cu and Ni being less than 0.02 wt.%.
The preparation method of the magnesium rare earth alloy in the comparative example is basically the same as that of the example 4, and the difference is only that: in the comparative example, the alloy is not subjected to thermal deformation treatment after smelting, and is directly subjected to aging treatment.
The mechanical properties of the magnesium rare earth alloy prepared by the comparative example are as follows: room temperature: the yield strength is 280.6MPa, the tensile strength is 300.9MPa, and the elongation is 2.3%. High temperature 150 ℃ of: the yield strength is 260.4MPa, the tensile strength is 290.8MPa, and the elongation is 5.8%.
Comparative example 4
The comparative example provides a magnesium rare earth alloy, which is basically consistent with example 4 in all the components in percentage by mass, and is different only in that: in the comparative example, the Ag element is adopted to replace Ho, and the Ag element comprises the following components in percentage by mass: 4 wt.% Gd, 2 wt.% Er, 0.2 wt.% Y, 4 wt.% Ag, 0.1 wt.% Zr, the balance Mg and unavoidable impurities, the total amount of impurity elements Si, Fe, Cu and Ni being less than 0.02 wt.%. The preparation method of the magnesium rare earth alloy in the comparative example is consistent with that of example 4.
The mechanical properties of the magnesium rare earth alloy prepared by the comparative example are as follows: room temperature: the yield strength was 300.9MPa, the tensile strength was 310.4MPa, and the elongation was 2.1%. High temperature 150 ℃ of: the yield strength was 287.6MPa, the tensile strength was 296.4MPa, and the elongation was 3.3%.
Comparative example 5
The comparative example provides a magnesium rare earth alloy, which is basically consistent with example 4 in all the components in percentage by mass, and is different only in that: in the comparative example, the mass percent of Er is 1 wt.%, namely, the mass percent of each component is as follows: 4 wt.% Gd, 1 wt.% Er, 0.2 wt.% Y, 4 wt.% Ho, 0.1 wt.% Zr, the balance Mg and unavoidable impurities, the total amount of impurity elements Si, Fe, Cu and Ni being less than 0.02 wt.%. The preparation method of the magnesium rare earth alloy in the comparative example is consistent with that of example 4.
The mechanical properties of the magnesium rare earth alloy prepared by the comparative example are as follows: room temperature: the yield strength is 274.9MPa, the tensile strength is 306.5MPa, and the elongation is 6.4%. High temperature 150 ℃ of: the yield strength is 247.8MPa, the tensile strength is 260.1MPa, and the elongation is 8.9%.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention. The embodiments and features of the embodiments of the present application may be combined with each other arbitrarily without conflict.

Claims (6)

1. The high-strength Mg-Gd-Er-Y magnesium alloy is characterized by comprising the following elements in percentage by weight: gd is 4-15 wt.%, Er is 2-6 wt.%, Y is 0.2-6 wt.%, Ho is 0-4 wt.%, Zr is 0-1 wt.%, and the total amount of Gd, Er, Y and Ho is: 6.2-20 wt.%, the balance being Mg and unavoidable impurities;
the preparation method of the high-strength Mg-Gd-Er-Y magnesium alloy comprises the steps of smelting, thermal deformation treatment and aging treatment in sequence;
the thermal deformation treatment comprises the following specific steps:
a1, carrying out solid solution on the alloy ingot obtained by smelting at 480-540 ℃ for 2-10 hours in advance, and quenching with warm water at 70 ℃;
a2, carrying out hot extrusion on the cast ingot subjected to the solution treatment in the step A1, wherein the extrusion temperature is 200 ℃, and the extrusion ratio is 20: 1;
the aging treatment comprises the following specific steps: aging for 2-10 h at 170-250 ℃, and then aging for 10-60 h at 100-170 ℃.
2. The high strength Mg-Gd-Er-Y magnesium alloy according to claim 1, wherein Ho in the magnesium alloy is 0.5-2 wt.%.
3. The high strength Mg-Gd-Er-Y magnesium alloy according to claim 1, wherein Zr in the magnesium alloy is 0.5-1 wt.%.
4. The preparation method of the high-strength Mg-Gd-Er-Y magnesium alloy according to the claim 1, which is characterized by comprising three processes of smelting, thermal deformation treatment and aging treatment in sequence.
5. The preparation method of the high-strength Mg-Gd-Er-Y magnesium alloy according to claim 4, characterized in that the smelting comprises the following specific steps:
s1, baking materials: preheating pure magnesium and intermediate alloys of magnesium-gadolinium, magnesium-erbium, magnesium-yttrium, magnesium-holmium and magnesium-zirconium at the temperature of 200-240 ℃;
s2, melting magnesium, adding Gd, Er, Y and Ho: melting the dried pure magnesium in a protective atmosphere; after pure magnesium is completely melted, adding Mg-Gd intermediate alloy, Mg-Er intermediate alloy, Mg-Y intermediate alloy and Mg-Ho intermediate alloy when the temperature of the melt is raised to 730-750 ℃;
s3, adding Zr: adding Mg-Zr intermediate alloy when the temperature of the melt obtained in the step S2 reaches 750-780 ℃ in a protective atmosphere;
s4, casting: and under a protective atmosphere, stirring when all alloys are completely melted and the temperature of the melt rises to 730-750 ℃, then refining without power failure for 5-10 minutes when the temperature of the melt rises to 750-760 ℃, heating to 780 ℃ after refining, standing for 25-40 minutes, skimming the surface scum after the melt is cooled to 710-740 ℃ after standing, and casting to obtain the alloy ingot.
6. The preparation method of the high-strength Mg-Gd-Er-Y magnesium alloy according to the claim 5, characterized in that in the step S2, after the pure magnesium is completely melted, the Mg-Gd intermediate alloy, the Mg-Er intermediate alloy, the Mg-Y intermediate alloy and the Mg-Ho intermediate alloy are added in sequence when the melt temperature is raised to 730-750 ℃.
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